Shale reservoir space hydrophilic characteristic evaluation device and method under different water content conditions
By designing closed experimental devices and automatic control technology, the accuracy of water storage space characteristics evaluation in the humidity stage of shale reservoir is solved, and the hydrophilic characteristics of shale reservoirs are quantitatively evaluated, and the accuracy of gas content evaluation of shale reservoirs is improved.
Patent Information
- Application Number
- CN202410139884.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-02-01
- Publication Date
- 2025-08-01
AI Technical Summary
The prior art cannot accurately evaluate the water storage space characteristics of different relative humidity stages of shale reservoirs without external interference, resulting in inaccurate evaluation of gas content in shale reservoirs.
A closed experimental device is designed, including a sample preparation area, a saturated solution area and a gas adsorption area, a temperature control unit and a robotic arm are installed to achieve relative humidity equilibrium and automatic control of the gas adsorption process, and sample transfer and gas measurement are performed through quantitative manifolds and dewar tanks.
The quantitative evaluation of the hydrophilic characteristics of shale storage space in a closed environment is achieved, experimental errors are avoided, and the characteristics of water storage space at different humidity stages can be accurately characterized, providing theoretical support for the gas content of shale reservoirs.
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Figure CN120404489A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of oil and gas exploration, and particularly relates to an evaluation device and method for the hydrophilic characteristics of shale reservoir spaces under different water content conditions, which are mainly used for oil and gas exploration such as shale gas and shale oil. Background Art
[0002] The humidity equilibrium process of a saturated salt solution refers to the fact that ions in the salt solution hinder the evaporation of water molecules on the solution surface due to solvation. If the salt solution is in a closed container, the evaporation of water molecules in the solution reaches a relative equilibrium with the water molecules in the gas phase, and finally the relative humidity in the closed container reaches equilibrium. The physical adsorption process refers to the automatic aggregation of a certain adsorbate on the solid surface due to van der Waals forces, so that the concentration of the adsorbate on the solid surface is higher than that in its bulk, in order to obtain a tendency to reduce the surface energy. The physical adsorption analysis experiment uses gas molecules with a known molecular cross-sectional area as probes, and obtains the pore size distribution information of the adsorbent by comparing the corresponding relationship between the amount of gas adsorbed on a certain surface during the experiment and the relative pressure of the corresponding adsorbate. Combining the saturated salt solution humidity equilibrium experiment and physical adsorption is of great significance for studying the spatial distribution of water molecules in shale reservoirs under different relative humidity conditions. And the water content is an important factor affecting the gas content of shale. Evaluating the spatial distribution of water molecules in shale reservoirs under different water saturation conditions provides theoretical support for accurately evaluating the gas content of shale reservoirs.
[0003] At present, most of the measurement methods for evaluating the water storage space characteristics of shale at different relative humidity stages cannot achieve in-situ measurement, and are greatly interfered by experimental errors, which limits the research on the water storage space of shale and thus affects the accurate evaluation of the gas content of shale reservoirs. Most of the existing studies on the water storage space of shale at different relative humidity stages only combine the saturated salt solution humidity equilibrium experiment and the physical adsorption experiment from the experimental process. And currently, when studying the water storage space characteristics of shale at different relative humidity stages, most of them use a shale sample divided into multiple parts, and conduct saturated salt solution humidity equilibrium experiments respectively based on different preset relative humidity conditions, and then conduct physical adsorption experiments on the shale samples respectively. Due to the extremely strong heterogeneity of shale, the existing experimental methods cannot accurately characterize the water storage space characteristics of shale at different humidity stages, and the experimental results are greatly interfered by the external environment. During the experiment, since the relative humidity state of the sample changes when the sample is transferred between experimental devices, and the experimental environment interference will also greatly affect the accuracy of the research on the reservoir space characteristics of shale at different relative humidity stages.
[0004] Therefore, a new device and method are needed to quantitatively evaluate the hydrophilic characteristics of the reservoir space of shale samples under different water saturation conditions while avoiding external interference. Summary of the Invention
[0005] The present application provides a device and method for evaluating the hydrophilic characteristics of shale reservoir space under different water-containing conditions to solve the above-mentioned technical problems that the experimental devices / methods in the prior art cannot be based on the original sample and the experimental disturbance is extremely large.
[0006] According to one aspect of the present application, an embodiment provides a device for evaluating the hydrophilic characteristics of shale reservoir space under different water-containing conditions, including an experimental area; the experimental area includes:
[0007] The sample preparation area is used to grind and prepare samples with a preset particle size;
[0008] a saturated solution zone, for preparing a solution of the solute and the solvent based on a preset relative humidity, and causing the saturated solution zone to reach a relative humidity equilibrium process; and
[0009] Gas adsorption area;
[0010] The sample preparation area, the saturated solution area, and the gas adsorption area are all configured as closed spaces, and a temperature control unit for controlling the temperature in the closed space is provided in each of the closed spaces; and an opening and closing door for experimental instruments to pass through is provided between two adjacent closed spaces.
[0011] Wherein, the gas adsorption area includes:
[0012] A sample transfer tank is used to transfer the sample from the saturated solution area to the gas adsorption area;
[0013] The retractable robotic arm b is used to transfer the sample tube containing the sample to the bottom of the quantitative manifold, wherein the sample tube cooperates with the bottom of the sample transfer tank to collect the sample;
[0014] a quantitative manifold, used for introducing gas into the sample tube;
[0015] a Dewar tank fixed below the quantitative manifold; and
[0016] The measuring element is used to measure the pressure of the sample tube and the manifold temperature after the pressure is balanced between the sample tube and the quantitative manifold.
[0017] In one embodiment, the sample preparation area has a portion for fixing a metal sieve plate and a retractable vibrating grinding pestle; the retractable vibrating grinding pestle is used to grind the sample on the top metal sieve plate, and the bottom metal sieve plate is used to collect powdered rock samples; wherein, the mesh sizes of the top metal sieve plate and the bottom metal sieve plate match the mesh sizes of the powdered rock samples to collect powdered rock samples that meet the mesh size requirements.
[0018] In one embodiment, the saturated solution area includes a solute tank and a solvent tank; in the saturated solution area, a fixed amount of solute and solvent are added to the solution tank to prepare a solution; and a stirrer is provided in the saturated solution area for stirring the solution to accelerate the relative humidity balance process in the saturated solution area.
[0019] In one embodiment, the experimental area includes a sieve sample plate storage area; the sieve sample plate storage area is set as the closed space, and a temperature control unit for controlling the temperature in the closed space to be constant is set in the closed space; the sieve sample plate storage area is adjacent to the sample preparation area, and the opening and closing door is opened on the sieve sample plate storage area.
[0020] In one embodiment, the experimental area includes a sample drying area; the sample drying area is set as the enclosed space, and a temperature control unit for controlling the constant temperature in the enclosed space and a retractable robotic arm a for transferring the sample clamp from the sample drying area are provided in the enclosed space; the opening and closing door is provided on the sample drying area; and the sample drying area is connected to an external vacuum pump a.
[0021] In one embodiment, the device for evaluating the hydrophilic characteristics of shale reservoir space under different water-containing conditions includes a transition zone; the transition zone is adjacent to at least one closed space in the experimental area; a control door is provided on the transition zone, and the transition zone is used for transition when samples are transferred between different closed spaces; a temperature control unit is provided in the transition zone for controlling the temperature in the closed space to be constant.
[0022] In one embodiment, the device for evaluating the hydrophilic characteristics of shale reservoir space under different water-containing conditions includes a cleaning area with a control door; the cleaning area is used to receive and clean experimental equipment that is in direct contact with the sample; the cleaning area includes a cleaning tank and a fixed ultrasonic transducer; the bottom of the cleaning tank is connected to a drainer, which is connected to a waste liquid collection area; the bottom of the cleaning tank is connected to a supplier, which is connected to a detergent supply area.
[0023] In one embodiment, the temperature control unit includes a constant temperature controller, a temperature sensor and a heater.
[0024] In one embodiment, the gas adsorption zone is connected to an external vacuum pump b; and / or,
[0025] The quantitative manifold connects the adsorbate gas container and the free space measurement gas container.
[0026] In one embodiment, the sample tube includes an outer sample tube; the outer sample tube has a spherical container, and the spherical container is fixedly connected to a neck; a filling column is inserted into the outer sample tube, the neck has an opening, and the opening is provided with a sample tube opening and closing door.
[0027] According to one aspect of the present application, an embodiment provides a method for evaluating the hydrophilic characteristics of shale reservoir spaces under different water-containing conditions, comprising the following steps:
[0028] S1. In the sample preparation area, grind the sample placed on the metal sieve template a; wherein, the required mesh number of the rock powder sample is Ms1 to Ms2, and two metal sieve templates are fixed in the sample preparation area, the upper limit of the mesh number conforms to the range value Ms1 of the metal sieve template a, and the lower limit of the mesh number conforms to the range value Ms2 of the metal sieve template b;
[0029] S2. The powdered rock sample meeting the mesh number requirements passes through the metal sieve template a and is concentrated on the metal sieve template b; record the mass of the rock powder sample as m1, wherein, a micro gravity sensor is attached to the metal sieve template b;
[0030] S3. In the saturated solution area, add a quantitative solute and solvent to the solution tank to prepare a solution, and set a preset humidity RH1; the metal sieve template b enters the saturated solution area and seals the saturated solution area until the humidity reaches RH1 again;
[0031] S4. The sample transfer tank enters the saturated solution area to snap and fix the metal sieve template b, and the sample transfer tank returns the metal sieve template b to the gas adsorption area;
[0032] S5. The sample transfer tank is flipped, the sample drops and is collected into the sample tube; the telescopic robotic arm b transfers the sample tube containing the sample to below the quantitative manifold and fixes it; add coolant to the Dewar tank;
[0033] S6. Charge a quantitative free space measurement gas into the quantitative manifold, and record this pressure as P m and the manifold temperature T m ; Open the quantitative manifold again, so that the free space measurement gas inside the quantitative manifold is charged into the sample tube, and record this pressure as P m ’ and the manifold temperature T m ’ ;
[0034] S7. Charge an adsorbate gas into the quantitative manifold, and record this pressure as P1 and the manifold temperature T1; Open the quantitative manifold again, so that the adsorbate gas inside the quantitative manifold is charged into the sample tube, and record this pressure as P1' and the manifold temperature T1';
[0035] S8. According to the free space measurement gas pressure data, the free space is determined by the linear relationship between the volume of the free space measurement gas supplied to the sample tube and the final equilibrium pressure, and there is:
[0036]
[0037] Where: V di is the gas supply volume at a certain data point, V di-1 is the gas supply volume at the previous data point, T std is the standard state temperature of the gas, P std is the standard state pressure of the gas, V m is the free space volume;
[0038] S9. Perform a linear regression on V di against P mi ', and the obtained slope and intercept are used to correct the free space volume and nitrogen adsorption data; where the volume of the adsorbate gas is:
[0039]
[0040] Where: V di is the gas supply volume at a certain data point, A F is the slope of the regression line of the free space measurement gas, B F is the intercept of the regression line of the free space measurement gas, m1 is the mass of the rock powder sample, P i ' is the pressure when the adsorbate gas fills the sample tube and reaches equilibrium;
[0041] S10. Repeat the gas adsorption experiment and calculate the adsorption amount at each pressure point corresponding to the humidity RH1.
[0042] In one embodiment, the method for evaluating the hydrophilic characteristics of the shale reservoir space under different water-containing conditions includes the following steps:
[0043] S11. After a certain experiment is completed, the retractable robotic arm b retrieves the sample tube and places it on the sample transfer groove. The sample transfer groove flips, and the sample is placed back on the metal sieve template b; set a preset temperature 1 and continuously dry the sample;
[0044] S12. Drain the solution in the solution tank; according to the preset humidity RH2, through the combined control of the solute addition port and the solvent addition port, add the solute and solvent that meet RH2 to the solution tank;
[0045] S13. Move the metal sieve template b to the saturated solution area until the humidity reaches RH2; repeat the adsorption experiment to obtain the adsorption amount V 2i ' corresponding to RH2;
[0046] S14. Repeat the adsorption experiment multiple times to obtain the adsorption amount V n corresponding to each pressure point of RH ni ’ ;
[0047] S15. Calculate the hydrophilic space parameter RW at different relative humidity stagesn ,
[0048]
[0049] Where: V′ nimax is the maximum adsorption volume measured, and LN(RH n ) is the natural logarithm of the relative humidity.
[0050] The technical solution of the above embodiments of the present application has the following advantages:
[0051] 1. This technical solution realizes the automatic control of the relative humidity balance process and the gas adsorption process, eliminates the influence of human operation delay factors on the experimental process, and the entire shale reservoir space hydrophilic characteristic evaluation device under different water content conditions is in a closed environment during the experiment, avoiding experimental errors caused by environmental changes during the experiment.
[0052] 2. This technical solution can quantitatively evaluate the hydrophilic characteristics of the shale reservoir space at different humidity stages, find out the differences in the water absorption capacity provided by different hydrophilic components in shale samples at different water content stages, and can realize the original sample research in the true sense, with practical statistical research significance.
[0053] 3. The research results of this technical solution have important theoretical significance for quantitatively evaluating the differences in the overall water absorption capacity of different shale components under different water content conditions, and have important practical significance for quantitatively evaluating the gas content in shale under different water content conditions.
[0054] 4. This technical solution can realize the research on the characteristics of the shale reservoir space at different humidity stages. During the actual research process, the sample specifications can be selected according to the actual research needs, which better meets the needs of actual production research. At the same time, the original sample research also avoids the influence of heterogeneity. BRIEF DESCRIPTION OF THE DRAWINGS
[0055] Figure 1 is a front view structural schematic diagram of a shale reservoir space hydrophilic characteristic evaluation device under different water content conditions in an embodiment;
[0056] Figure 2 is a rear view structural schematic diagram of a shale reservoir space hydrophilic characteristic evaluation device under different water content conditions in an embodiment;
[0057] Figure 3 is a structural schematic diagram of a sample clamp in an embodiment;
[0058] Reference numerals:
[0059] Ⅰ - Experimental area; Ⅱ - Transition area; Ⅲ - Cleaning area;
[0060] 1-sample drying area; 2-sieve sample storage area; 3-sample preparation area; 4-saturated solution area; 5-gas adsorption area; 8-sample tube;
[0061] 11-Opening and closing door A; 12-Sample holder opening and closing door; 13-External vacuum pump a; 14-Temperature sensor a; 15-Thermostatic controller a; 16-Heating element a; 17-Opening and closing door a; 18-Retractable robotic arm a; 19-Sample holder;
[0062] 21-opening and closing door B; 22-temperature sensor b; 23-heater b; 24-thermostat b;
[0063] 31 - residual sample tank; 32 - residual sample tank opening and closing door; 33 - metal sieve sample plate b; 34 - metal sieve sample plate a; 35 - opening and closing door C; 36 - retractable vibrating grinding pestle; 37 - temperature sensor c; 38 - constant temperature controller c; 39 - heater c;
[0064] 41 - solution tank; 42 - stirrer; 43 - drain port a; 44 - opening and closing door D; 45 - solute addition port; 46 - solvent addition port; 47 - solute tank; 48 - solvent tank; 49 - temperature sensor d; 410 - humidity sensor; 411 - constant temperature controller d; 412 - heater d;
[0065] 51 - Sample storage tank; 52 - Supply port; 53 - Liquid level monitor; 54 - Liquid inlet; 55 - Liquid level replenisher; 56 - Temperature sensor f; 57 - Retraction door; 58 - Dewar tank; 59 - Quantitative manifold; 511 - Retractable robotic arm b; 512 - Connector b; 513 - Sample transfer tank; 514 - Connector a; 515 - Temperature sensor e; 516 - Constant temperature controller e; 517 - Heater e; 518 - Coolant supply tank; 519 - Free space measurement gas container; 520 - Adsorbate gas container; 521 - External vacuum pump b;
[0066] 61-control door A; 62-control door B; 63-temperature sensor g; 64-heater g; 65-thermostat g;
[0067] 71 - waste liquid collection area; 72 - detergent supply area; 73 - drainer; 74 - supply; 75 - drain port b; 76 - ultrasonic transducer; 77 - cleaning tank; 78 - conversion bayonet; 79 - control door D; 710 - control door C;
[0068] 81 - external sample tube; 82 - packing column; 83 - sample tube opening and closing door. DETAILED DESCRIPTION
[0069] It should be noted that, without conflict, the embodiments in the present application and the features in the embodiments may be combined with each other. The present application will be described in detail below with reference to the accompanying drawings and in combination with the embodiments.
[0070] In order to enable those skilled in the art of this technology to better understand the solution of the present application, the technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present application. Obviously, the described embodiments are only a part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present application.
[0071] It should be noted that the terms "first", "second", etc. in the present application are used to distinguish similar objects, and do not have to be used to describe a specific order or sequence. It should be understood that such used data can be interchanged under appropriate circumstances, so as to describe the embodiments of the present application here. In addition, the terms "including" and "having" and any variations thereof are intended to cover non-exclusive inclusion. For example, a process, method, system, product or device including a series of steps or units does not have to be limited to those steps or units clearly listed, but may include other steps or units not clearly listed or inherent to these processes, methods, products or devices.
[0072] It should be understood that when an element (such as a layer, film, region, or substrate) is described as being "on" another element, the element can be directly on the other element, or there may also be an intermediate element. Moreover, in the present application, when it is described that an element is "connected" to another element, the element can be "directly connected" to the other element, or "connected" to the other element through a third element.
[0073] Embodiment 1
[0074] Please refer to Figure 1-Figure 3, An embodiment provides an evaluation device for the hydrophilic characteristics of shale reservoir spaces under different water-containing conditions, including Experimental Area I; the Experimental Area I includes: a sample preparation area 3, a saturated solution area 4, and a gas adsorption area 5; wherein, the sample preparation area 3 is used for grinding and preparing samples with a preset particle size; the saturated solution area 4 is used for preparing a solution by mixing a solute and a solvent based on a preset relative humidity and promoting the relative humidity balance process in the saturated solution area 4. Among them, the sample preparation area 3, the saturated solution area 4, and the gas adsorption area 5 are all set as closed spaces, and a temperature control unit for keeping the temperature constant in the closed space is provided in each of the closed spaces; an opening and closing door for the passage of experimental instruments is provided between two adjacent closed spaces. Specifically, the gas adsorption area 5 includes: a sample transfer groove 513, a telescopic robotic arm b511, a quantitative manifold 59, a Dewar tank 58, and a measuring element; wherein, the sample transfer groove 513 is used for transferring the sample from the saturated solution area 4 to the gas adsorption area 5; the telescopic robotic arm b511 is used for transferring the sample tube 8 containing the sample below the quantitative manifold 59, wherein the sample tube 8 cooperates with the bottom of the sample transfer groove 513 to collect the sample; the quantitative manifold 59 is used for introducing gas into the sample tube 8; the Dewar tank 58 is fixed below the quantitative manifold 59; the measuring element is used for measuring the pressure after the pressure balance between the sample tube 8 and the quantitative manifold 59 and the manifold temperature.
[0075] In one embodiment, the part of the sample preparation area 3 with a fixed metal sieve template and a telescopic vibrating pestle 36; the telescopic vibrating pestle 36 is used for grinding the sample on the top metal sieve template, and the bottom metal sieve template is used for collecting the powdered rock sample; wherein, the mesh numbers of the top metal sieve template and the bottom metal sieve template match the mesh number of the powdered rock sample to collect the powdered rock sample meeting the mesh number requirements. In a specific example, the telescopic vibrating pestle 36 acts jointly with the preset specification metal sieve template a34 and the metal sieve template b33 moved to the sample preparation area 3 to grind and prepare a sample with a preset particle size. The remaining sample groove 31 is used to accommodate the remaining sample, and there is an opening and closing door at the bottom of the remaining sample groove 31 for transferring the remaining sample. Specifically, according to the required mesh number requirements (Ms1~Ms2) of the rock powder sample, two suitable metal sieve templates are selected from the sieve template storage area 2, and the metal sieve templates are moved to the sample preparation area 3 through the chute, so that the upper limit of the mesh number conforms to the range value Ms1 of the sieve template a, and the lower limit of the mesh number conforms to the range value Ms2 of the sieve template b. The telescopic vibrating pestle 36 extends and vibrates to grind the sample. The powdered rock sample meeting the mesh number requirements passes through the metal sieve template a34 and accumulates on the metal sieve template b33. A micro gravity sensor is attached to the metal sieve template. When the rock powder on the metal sieve template b33 reaches the preset value, the telescopic vibrating pestle 36 stops grinding, and the computer records the mass of the rock powder sample.
[0076] In one embodiment, the saturated solution area 4 includes a solute tank 47 and a solvent tank 48; in the saturated solution area 4, a certain amount of solute and solvent are added to the solution tank 41 to prepare a solution; a stirrer 42 is provided in the saturated solution area 4 for stirring the solution to accelerate the relative humidity equilibrium process in the saturated solution area 4. Specifically, the stirrer 42 continuously stirs the solution during the relative humidity equilibrium process to accelerate the relative humidity equilibrium process in the saturated solution area 4. The drain port in the saturated solution area 4 is used to drain the solution in the solution tank 41.
[0077] In one embodiment, the experimental area I includes a sieve template storage area 2; the sieve template storage area 2 is set as the enclosed space for storing metal sieve templates, and the metal sieve templates are transferred to the sample preparation area 3 to prepare rock powder samples; a temperature control unit for controlling the temperature in the enclosed space is provided in the enclosed space; the sieve template storage area 2 is adjacent to the sample preparation area 3, and the opening and closing door is provided on the sieve template storage area 2.
[0078] In one embodiment, the experimental area I includes a sample drying area 1; the sample drying area 1 is set as the enclosed space, and a temperature control unit for controlling the temperature in the enclosed space and a retractable robotic arm a18 for transferring the sample clamp 19 from the sample drying area 1 are provided in the enclosed space; the opening and closing door is provided on the sample drying area 1; the sample drying area 1 is connected to an external vacuum pump a. Among them, the retractable robotic arm a18 can control the transfer of the sample clamp 19 between different experimental areas. There is an opening and closing door 12 at the lower part of the sample clamp 19 for the transfer of samples. The external vacuum pump a13 is used to remove other gases inside the sample and maintain the entire closed device in a vacuum state.
[0079] In one embodiment, the device for evaluating the hydrophilic characteristics of shale reservoir spaces under different water content conditions includes a transition area II; the transition area II is adjacent to at least one enclosed space in the experimental area I; a control door is provided on the transition area II, and the transition area II is used for the transition when the sample is transferred between different enclosed spaces; a temperature control unit for controlling the temperature in the enclosed space is provided in the transition area II.
[0080] In one embodiment, the hydrophilic characteristic evaluation device for shale reservoir space under different water content conditions includes a cleaning area III with a control door; the cleaning area III is used to receive and clean the experimental instruments in direct contact with the sample; the cleaning area III includes a cleaning tank 77 and a fixedly arranged ultrasonic transducer 76; the bottom of the cleaning tank 77 is connected to a liquid drainer 73, and the liquid drainer 73 is connected to a waste liquid collection area 71; the liquid drain port b75 of the cleaning area III is connected to the liquid drain port a43 of the saturated solution area 4; the bottom of the cleaning tank 77 is connected to a feeder 74, and the feeder 74 is connected to a cleaning agent supply area 72. In the cleaning area III, the cleaning agent in the cleaning tank 77 and the ultrasonic transducer 76 work together to enable the experimental instruments in direct contact with the sample to be transferred to the cleaning tank 77 through a sliding groove for cleaning after each experiment.
[0081] In one embodiment, the temperature control unit includes a constant temperature controller, a temperature sensor, and a heater. The temperature control unit is used to control heating so that the temperature reaches a preset temperature 1 and a preset temperature 2. Since the temperature control unit is set in many places, the specific setting method is described in detail in Embodiment III.
[0082] In one embodiment, the gas adsorption area 5 is connected to an external vacuum pump b521; the quantitative manifold 59 is connected to an adsorbate gas container 520 and a free space measurement gas container 519. The external vacuum pump b521 is used for vacuum pumping. The adsorbate gas container 520 supplies adsorbate gas to the quantitative manifold 59, and the free space measurement gas container 519 supplies free space measurement gas to the quantitative manifold 59 for process measurement.
[0083] In one embodiment, the sample tube 8 includes an outer sample tube 81; the outer sample tube 81 has a spherical container, and the spherical container is fixedly connected with a neck; a filling column 82 is inserted into the outer sample tube 81, the neck has an opening, and a sample tube opening and closing door 83 is arranged at the opening. In a specific example, the sample transfer groove 513 is recessed towards the center, and the sample tube 8 is detachably connected to the center of the sample transfer groove 513 to facilitate collecting the powdered rock sample in the sample transfer groove 513.
[0084] The hydrophilic characteristic evaluation device for shale reservoir space under different water content conditions of the present application can construct a hydrophilic characteristic evaluation method for shale reservoir space under different water content conditions, and accurately evaluate the difference in reservoir space characteristics of shale under different relative humidity conditions through the study of hydrophilic characteristic parameters of the same shale sample under different humidity environments. The present invention overcomes the great disadvantages of the existing experimental methods that cannot be based on the original sample and experimental disturbance, and can quantitatively characterize the difference in reservoir space characteristics of shale under different relative humidity conditions, providing theoretical support for evaluating the gas content of shale reservoirs.
[0085] Embodiment II
[0086] Please refer to Figure 1-Figure 3 , an embodiment provides an evaluation device for the hydrophilic characteristics of shale reservoir spaces under different water content conditions. The following will elaborate on the technical solution of the present invention from the perspective of the inventor, which is conducive to those skilled in the art to familiarize themselves with the idea of the present invention. Among them, for some technical key points, detailed explanations are provided in order to enable those skilled in the art to comprehensively understand the technical solution of the present invention.
[0087] An evaluation device for the hydrophilic characteristics of shale reservoir spaces under different water content conditions is a device that controls the humidity (water saturation) of shale and measures relevant parameters, including experimental area I, transition area II, cleaning area III, and a control device. This evaluation device is connected to a computer and can run data recording software related to the evaluation of the hydrophilic characteristics of shale reservoir spaces under different water content conditions.
[0088] Experimental area I includes a sample drying area 1, a sieve plate storage area 2, a sample preparation area 3, a saturated solution area 4, and a gas adsorption area 5.
[0089] 1. The sample drying area 1 includes a constant temperature controller a15, a temperature sensor a14, a heater a16, an opening and closing door a17, a telescopic robotic arm a18, a sample clamp 19, an opening and closing door A11, and an external vacuum pump a13.
[0090] Among them, the temperature sensor a14 is used to sense the temperature inside the sample drying area 1. The heater a16 is controlled by the constant temperature controller a15 to adjust the temperature of the sample drying area 1 to be constant at a preset drying temperature. The telescopic robotic arm a18 can control the sample clamp 19 to transfer between different experimental areas. There is an opening and closing door 12 at the lower part of the sample clamp 19 for sample transfer. The external vacuum pump a13 is used to remove other gases inside the sample and maintain the entire closed device in a vacuum state.
[0091] 2. The sieve plate storage area 2 includes a constant temperature controller b24, a temperature sensor b22, a heater b23, metal sieve plates of various specifications, and an opening and closing door B21.
[0092] Among them, the temperature sensor b22 is used to sense the temperature inside the sieve plate storage area 2. The heater b23 is controlled by the constant temperature controller b24 to adjust the temperature of the sieve plate storage area 2 to a constant temperature. Tiny gravity sensors are attached to the edges of the metal sieve plates, and the accuracy of the gravity sensors can reach 0.01 mg.
[0093] 3. The sample preparation area 3 includes a constant temperature controller c38, a temperature sensor c37, a heater c39, a telescopic vibrating grinding pestle 36, a waste sample trough 31, and an opening and closing door C35.
[0094] Among them, the temperature sensor c37 is used to sense the temperature in the sample preparation area 3. The heater c39 is controlled by the constant temperature controller c38 to adjust the temperature in the sample preparation area 3 to a constant temperature. The retractable vibrating grinding pestle 36 acts jointly with the preset specification metal sieve templates a34 and b33 moved to the sample preparation area 3 to grind and prepare samples with a preset particle size. The remaining sample tank 31 is used to hold the remaining samples, and there is an opening / closing door 32 at the bottom of the remaining sample tank 31 to transfer the remaining samples.
[0095] 4. The saturated solution area 4 includes a constant temperature controller d411, a temperature sensor d49, a heater d412, a humidity sensor 410, a solute tank 47, a solute addition port 45, a solvent tank 48, a solvent addition port 46, a solution tank 41, a drain port a43, a stirrer 42, and an opening / closing door D44.
[0096] Among them, the temperature sensor d49 is used to sense the temperature in the saturated solution area 4. The heater d412 is controlled by the constant temperature controller d411 to adjust the temperature in the saturated solution area 4 to a constant temperature. The solute tank 47 storing various solutes and the solvent tank 48 storing various solvents act jointly to add a certain amount of solute and solvent to the solution tank 41 based on a preset relative humidity. The stirrer 42 continuously stirs the solution during the relative humidity balancing process to accelerate the relative humidity balancing process in the saturated solution area 4. The drain port is used to drain the solution in the solution tank 41.
[0097] 5. The gas adsorption area 5 includes a constant temperature controller e516, a temperature sensor e515, a heater e517, a sample transfer tank 513, a sample tube 8, a connection port a514, a connection port b512, a retractable robotic arm b511, a quantitative manifold 59, a Dewar tank 58, a temperature sensor f56, a liquid level monitor 53, a liquid inlet 54, a supply port 52, a coolant supply tank 518, a sample storage tank 51, an external vacuum pump b521, an adsorbate gas container 520, and a free space measurement gas container 519.
[0098] Among them, the temperature sensor e515 is used to sense the temperature in the gas adsorption zone 5. The heater e517 is controlled by the constant temperature controller e516 to adjust the temperature in the gas adsorption zone 5 to a constant temperature. The sample transfer slot 513 is flipped with the connection port a514 and the connection port b512 as fixed points to transfer the sample into / out of the sample tube 8. The sample tube 8 is composed of an outer sample tube 81, a packing column 82 and a sample tube opening / closing door 83. The packing column 82 is used to minimize the free space inside the sample tube 8 and improve the accuracy of the test. The sample tube opening / closing door 83 can be closed during sample transfer to ensure that the humidity remains unchanged during sample transfer. The telescopic robotic arm b511 can control the transfer of the sample tube 8 within the gas adsorption zone 5. The quantitative manifold 59 can quantitatively control the amount of gas entering the sample tube 8. There is a retractable door 57 on the upper part of the Dewar tank 58, with a temperature sensor f56 and a liquid level monitor 53 built in. The retractable door 57 on the upper part of the Dewar tank 58 can be retracted and closed to isolate the inside of the Dewar tank 58 from the outside. The temperature sensor f56 is used to measure the real-time temperature inside the coolant and send the temperature to the computer, and the computer can obtain the corresponding saturated vapor pressure through a program. The liquid level replenisher 55 and the liquid level monitor 53 can control the height of the coolant inside the Dewar tank 58 according to the set liquid level height. The sample storage tank 51 is used to store the samples after the experiment is completed.
[0099] 6. The transition zone II includes a constant temperature controller g65, a temperature sensor g63, a heater g64, a control door A61 and a control door B62. The transition zone II is used for the transition of the sample when transferring between different regions.
[0100] Among them, the temperature sensor g63 is used to sense the temperature in the transition zone II. The heater g64 is controlled by the constant temperature controller g65 to adjust the temperature in the transition zone II to a constant temperature.
[0101] 7. The cleaning zone III includes a cleaning tank 77, a conversion bayonet 78, a control door C710, a control door D79, an ultrasonic transducer 76, a liquid drainer 73, a liquid drain port b75, a feeder 74, a waste liquid collection area 71 and a cleaning agent supply area 72.
[0102] Among them, the liquid drain port b75 in the cleaning zone III is connected to the liquid drain port a43 in the saturated solution zone 4. The cleaning agent in the cleaning tank 77 and the ultrasonic transducer 76 work together to clean the experimental apparatus in direct contact with the sample by transferring it to the cleaning tank 77 through the chute after each experiment.
[0103] Example 3
[0104] An embodiment provides a method for evaluating the hydrophilic characteristics of shale reservoir spaces under different water content conditions. Among them, the method for evaluating the hydrophilic characteristics of shale reservoir spaces under different water content conditions can be applied to the device for evaluating the hydrophilic characteristics of shale reservoir spaces under different water content conditions. The following is an explanation in combination with the device for evaluating the hydrophilic characteristics of shale reservoir spaces under different water content conditions.
[0105] A method for evaluating the hydrophilic characteristics of shale reservoir spaces under different water content conditions, comprising the following steps:
[0106] S1. In the sample preparation area 3, grind the sample placed on the metal sieve plate a34; wherein, the required mesh number of the rock powder sample is Ms1 to Ms2, and two metal sieve plates are fixed in the sample preparation area 3, the upper limit of the mesh number conforms to the range value Ms1 of the metal sieve plate a34, and the lower limit of the mesh number conforms to the range value Ms2 of the metal sieve plate b33;
[0107] S2. The powdered rock sample meeting the mesh number requirements passes through the metal sieve plate a34 and accumulates on the metal sieve plate b33; record the mass of the rock powder sample as m1, wherein, a micro gravity sensor is attached to the metal sieve plate b33;
[0108] S3. In the saturated solution area 4, add a quantitative solute and solvent to the solution tank 41 to prepare a solution, and set a preset humidity RH1; the metal sieve plate b33 enters the saturated solution area 4 and seals the saturated solution area 4 until the humidity reaches RH1 again;
[0109] S4. The sample transfer tank 513 enters the saturated solution area 4 to snap and fix the metal sieve plate b33, and the sample transfer tank 513 returns to the gas adsorption area 5 with the metal sieve plate b33;
[0110] S5. The sample transfer tank 513 is flipped, the sample drops and is collected into the sample tube 8; the retractable robotic arm b511 transfers the sample tube 8 containing the sample to below the quantitative manifold 59 and fixes it; add coolant to the Dewar tank 58;
[0111] S6. Charge a quantitative free space measurement gas into the quantitative manifold 59, and record this pressure as P m and the manifold temperature T m ; Open the quantitative manifold 59 again, so that the free space measurement gas inside the quantitative manifold 59 is charged into the sample tube 8, and record this pressure as P m ’ and the manifold temperature T m ’;
[0112] S7. Charge an adsorbate gas into the quantitative manifold 59, and record this pressure as P1 and the manifold temperature T1; Open the quantitative manifold 59 again, so that the adsorbate gas inside the quantitative manifold 59 is charged into the sample tube 8, and record this pressure as P1’ and the manifold temperature T1’ after the pressure reaches equilibrium;
[0113] S8. According to the free space measurement gas pressure data, the free space is determined by the linear relationship between the volume of the free space measurement gas supplied to the sample tube 8 and the final equilibrium pressure, and there is:
[0114]
[0115] Where: i For a data point, i-1 is the previous data point, V di is the gas supply volume at a certain data point, V di-1 is the gas supply volume of the previous data point, T std is the standard state temperature of the gas, P std is the standard pressure of the gas, V m is the volume of free space;
[0116] S9. V di P mi 'Perform linear regression, and the slope and intercept obtained are used to correct the free space volume and nitrogen adsorption data; where the volume of the adsorbate gas is:
[0117]
[0118] Where: V di is the gas supply volume at a certain data point, A F is the slope of the gas regression line measured in free space, B F is the intercept of the gas regression line measured in free space, m1 is the mass of the rock powder sample, P i ' is the pressure when the adsorbate gas is filled into the sample tube and reaches equilibrium;
[0119] S10. Repeat the gas adsorption experiment and calculate the adsorption amount at each pressure point corresponding to the humidity RH1;
[0120] S11. After an experiment is completed, the retractable robotic arm b511 retrieves the sample tube 8 and places it on the sample transfer tank 513. The sample transfer tank 513 is flipped over and the sample is placed back on the metal sieve plate b33. The preset temperature is set to 1 and the sample is continuously dried.
[0121] S12. The solution tank 41 is discharged; according to the preset humidity RH2, by jointly controlling the role of the solute addition port 45 and the solvent addition port 46, the solute and solvent are added to the solution tank 41 in accordance with RH2;
[0122] S13. The metal sieve template b33 is moved to the saturated solution zone 4 until the humidity reaches RH2; repeat the adsorption experiment to obtain the adsorption amount V corresponding to each pressure point RH2 2i ';
[0123] S14. Repeat the adsorption experiment several times to obtain RH n The corresponding adsorption amount V at each pressure point ni ';
[0124] S15. Calculate the hydrophilic space parameter RW at different relative humidity stages n ,
[0125]
[0126] Where: V′ nimax is the measured maximum adsorption volume, and LN(RH n ) is the natural logarithm of the relative humidity.
[0127] The evaluation method for the hydrophilic characteristics of shale reservoir space under different water content conditions of the present application can quantitatively evaluate the hydrophilic characteristics of shale reservoir space at different humidity stages, identify the differences in the water absorption capacity provided by different hydrophilic components in shale samples at different water content stages, and can achieve true in-situ research, having practical statistical research significance. Moreover, it realizes the automatic control of the relative humidity balance process and the gas adsorption process, eliminating the influence of human operation delay factors on the experimental process. The entire evaluation device for the hydrophilic characteristics of shale reservoir space under different water content conditions is in a closed environment during the experiment, avoiding experimental errors caused by environmental changes during the experiment.
[0128] Example 4
[0129] An embodiment provides an evaluation method for the hydrophilic characteristics of shale reservoir space under different water content conditions. The following will elaborate on the technical solution of the present invention from the perspective of the inventor, which is conducive to those skilled in the art to familiarize themselves with the idea of the present invention. Among them, for some technical key points, detailed explanations are provided in order to enable those skilled in the art to comprehensively understand the technical solution of the present invention.
[0130] An evaluation method for the hydrophilic characteristics of shale reservoir space under different water content conditions includes the following steps:
[0131] First, open the opening and closing door a and place the sample in the sample clamp. Before the experiment starts, all the opening and closing doors and control doors in the device (which can be the evaluation device for the hydrophilic characteristics of shale reservoir space under different water content conditions in Example 1 or Example 2) except the opening and closing door of the sample clamp are in the open state. Under the action of the external vacuum pump a, the entire device is in a vacuum state. At this time, each temperature controller controls the temperature of the entire device at 25°C. Then, all the opening and closing doors and control doors are closed. Through the computer control of the constant temperature controller a, the heater a and the temperature sensor a work together to keep the temperature of the sample drying area at the preset temperature 1 (generally about 70°C) and continue to dry the sample for the preset time 1 (generally more than 48h).
[0132] After that, the opening and closing door B is opened (by computer). According to the required mesh number requirements (Ms1 - Ms2) of the rock powder sample, two suitable metal sieve plates are selected from the sieve plate storage area. The metal sieve plates are moved to the sample preparation area through the chute, so that the upper limit of the mesh number conforms to the range value Ms1 of the sieve plate a, and the lower limit of the mesh number conforms to the range value Ms2 of the sieve plate b. The opening and closing door B is closed. The computer controls the thermostat b in the sieve plate storage area. The heater b and the temperature sensor b work together to keep the temperature in the sieve plate storage area at the preset temperature 2 (generally about 25 °C).
[0133] Then, the opening and closing door A is opened (by computer). The telescopic robotic arm a moves the sample to the sample preparation area. The sample clamp opening and closing door is opened, and the sample is placed on the metal sieve plate a. The telescopic robotic arm retracts, and the opening and closing door A is closed.
[0134] Furthermore, the thermostat c is controlled (by computer). The heater c and the temperature sensor c work together to keep the temperature in the sample drying area at the preset temperature 2 (generally about 25 °C). The telescopic vibrating grinding pestle extends and vibrates to grind the sample. The powdered rock sample meeting the mesh number requirements passes through the metal sieve plate a and accumulates on the metal sieve plate b. A micro pressure sensor (preferably a micro gravity sensor) is attached to the metal sieve plate. When the rock powder on the metal sieve plate b reaches the preset value, the telescopic vibrating grinding pestle stops grinding. The computer records the mass of the rock powder sample as m1.
[0135] Next, the thermostat d is controlled (by computer). The heater d and the temperature sensor d work together to keep the temperature in the saturated solution area at the preset temperature 2 (generally about 25 °C). According to the preset humidity RH1, by jointly controlling the computer, the thermostat d, the heater d and the temperature sensor d work together to keep the temperature in the saturated solution area at the preset temperature 2 (generally about 25 °C). According to the preset humidity RH1, by jointly controlling the computer, the opening and closing door C is opened. The metal sieve plate b slides to the saturated solution area through the chute, and the opening and closing door C is closed. The stirrer in the solution tank runs until the humidity sensor reading reaches RH1 again.
[0136] After that, the opening and closing door D is controlled to be opened (by computer). The sample transfer tank slides to the saturated solution area through the chute. The sample transfer tank moves down through the slide rail and buckles with the metal sieve plate b. The sample transfer tank then slides back to the gas adsorption area through the chute. The opening and closing door D is closed.
[0137] Next, the sample tube opening and closing door is opened. The sample transfer tank is flipped, and the sample gathers in the sample tube. The sample tube opening and closing door is closed. The telescopic robotic arm b transfers the sample tube to be fixed under the quantitative manifold. The supply port and the inlet in the coolant supply tank work together to add coolant to the Dewar tank to the preset liquid level interface. The temperature sensor records the temperature in the Dewar tank as T.
[0138] After that, the quantitative free space measurement gas is filled into the quantitative manifold of the instrument, and this pressure is recorded as P after equilibrium m and the manifold temperature T m . Then, the quantitative manifold is opened through the computer, so that the free space measurement gas inside the quantitative manifold is filled into the sample tube, and this pressure is recorded as P m ' and the manifold temperature T m ' after the pressure reaches equilibrium. Repeat the above measurement steps, measure at least one more pressure point of the free space measurement gas sample, and then slowly remove the free space measurement gas in the sample tube by using the external vacuum pump b
[0139] Then, the adsorbate gas is filled into the quantitative manifold of the instrument, and this pressure is recorded as P1 and the manifold temperature T1 after equilibrium. Then, the quantitative manifold is opened through the computer, so that the adsorbate gas inside the quantitative manifold is filled into the sample tube, and this pressure is recorded as P1' and the manifold temperature T1' after the pressure reaches equilibrium. When the intake gas volume of the adsorbate gas is gradually increased and the intake gas pressure is at least 0.99×106 Pa (relative pressure is at least 0.99) for multiple times, this pressure is recorded as P n ' and the manifold temperature T n '.
[0140] Among them, according to the free space measurement gas pressure data, the free space can be determined by the linear relationship between the volume of the free space measurement gas supplied into the sample tube and the final equilibrium pressure. The gas supply volume is There is:
[0141]
[0142] In the formula: i Unchangedis a certain data point i-1 is the previous data point, V di is the gas supply volume of a certain data point, V di-1 is the gas supply volume of the previous data point, T std is the gas standard state temperature, P std is the gas standard state pressure, V m is the free space volume
[0143] And perform a linear regression on V di against P mi ', and the obtained slope and intercept are used to correct the free space volume and nitrogen adsorption data. The volume of the adsorbate gas is:
[0144]
[0145] In the formula: V di is the gas supply volume of a certain data point, A F is the slope of the regression line of the free space measurement gas, BF For intercept of the gas regression line in free space measurement, m1 is the mass of the rock powder sample, and P i ′ is the pressure when the adsorbate gas fills the sample tube and reaches equilibrium;
[0146] Repeat the gas adsorption experiment again, and calculate the adsorption amounts at each pressure point corresponding to the humidity RH1.
[0147] After the first experiment is completed, the retractable robotic arm b retrieves the sample tube and places it on the sample transfer slot. The sample transfer slot flips, and the sample is placed back on the metal sieve template b. Through computer control of the constant temperature controller e, the heater e and the temperature sensor e act jointly to keep the temperature in the sample drying area at the preset temperature 1 (generally about 70°), and dry the sample for the preset time 1 (generally more than 48h).
[0148] After that, the solution in the solution tank is discharged through the drain port. According to the preset humidity RH2, by jointly controlling the solute addition port and the solvent addition port, add the solute Su2 and the solvent Sv2 that meet RH2 into the solution tank.
[0149] After that, the opening and closing door D opens, and the metal sieve template b is transported to the saturated solution area through the slide rail. The opening and closing door D closes. The stirrer in the solution tank operates until the humidity sensor shows RH2. Repeat the adsorption experiment to obtain the adsorption amount V 2i ’ at each pressure point corresponding to RH2.
[0150] Repeat the adsorption experiment multiple times to obtain the adsorption amount V n ’ at each pressure point corresponding to RH ni ’.
[0151] Finally, calculate the hydrophilic space parameter RW n ,
[0152]
[0153] In the formula: V′ nimax is the measured maximum adsorption volume, and LN(RH n ) is the natural logarithm of the relative humidity.
[0154] By comparing the hydrophilic space parameters RW n at different relative humidity stages of the same sample, find out the differences in the water absorption capacities provided by different hydrophilic components in the shale sample at different water content stages. The higher the hydrophilic space parameter RW n , it indicates that the strong hydrophilic components in this water content stage provide more water absorption capacity. The hydrophilic space parameter RW nThe lower it is, it indicates that the weakly hydrophilic components also start to provide water absorption capacity in this water-bearing stage. The research results have important theoretical significance for quantitatively evaluating the differences in the overall water absorption capacity of different shale components under different water-bearing conditions, and have important practical significance for quantitatively evaluating the gas content in shale under different water-bearing conditions.
[0155] In one embodiment, after the experiment on the same sample is completed, the experimental instruments that are in direct contact with the powder sample, such as the sample tube, the retractable grinding pestle, and the metal sieve template, can be placed in the cleaning tank through the chute for cleaning to prepare for the next experiment.
[0156] In one embodiment, after testing multiple samples, the hydrophilic space parameter RW of different samples can also be compared under the same relative humidity condition to evaluate the strength of the water molecule storage capacity of different samples under a specific relative humidity condition.
[0157] In one embodiment, the method for evaluating the hydrophilic characteristics of the shale reservoir space under different water-bearing conditions in this embodiment can be applied to the device for evaluating the hydrophilic characteristics of the shale reservoir space under different water-bearing conditions.
[0158] Combined with the device for evaluating the hydrophilic characteristics of the shale reservoir space under different water-bearing conditions, the overall experiment is in an automated process after the sample is placed in the sample clamp. And the sample can be transferred between different experimental zones I through the retractable robotic arm and the chute. And the whole experiment process can be automatically controlled by a computer to realize the full-automatic control of the relative humidity balance process and the gas adsorption process, eliminating the influence of human operation delay factors on the experiment process. The whole device is in a closed environment during the experiment to avoid experimental errors caused by environmental changes during the experiment. Using the various parameters measured in this device, the hydrophilic space parameters under different water saturation degrees can be calculated:
[0159]
[0160] Using this parameter can characterize the differences in the water absorption capacity provided by different hydrophilic components in shale samples at different water-bearing stages. Specifically, the hydrophilic space parameter RW n The higher it is, it indicates that the strongly hydrophilic components provide more water absorption capacity in this water-bearing stage. The hydrophilic space parameter RW n The lower it is, it indicates that the weakly hydrophilic components also start to provide water absorption capacity.
[0161] The above are only the preferred embodiments of the present application and are not used to limit the present application. For those skilled in the art, various changes and modifications can be made to the present application. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application shall be included within the protection scope of the present application.
Claims
1. An evaluation device for the hydrophilic characteristics of shale reservoir spaces under different water-containing conditions, characterized in that It includes an experimental area; the experimental area includes: A sample preparation area for grinding and preparing samples with a preset particle size; A saturated solution area for preparing a solution of a solute and a solvent based on a preset relative humidity and promoting the relative humidity balance process in the saturated solution area; and A gas adsorption area; Among them, the sample preparation area, the saturated solution area, and the gas adsorption area are all set as enclosed spaces, and a temperature control unit for controlling the temperature in the enclosed space is provided in each enclosed space; an opening and closing door for experimental instruments to pass through is provided between two adjacent enclosed spaces; Among them, the gas adsorption area includes: A sample transfer groove for transferring samples from the saturated solution area to the gas adsorption area; A telescopic robotic arm b for transferring a sample tube containing a sample to below the quantitative manifold, where the sample tube cooperates with the bottom of the sample transfer groove to collect samples; A quantitative manifold for introducing gas into the sample tube; A Dewar tank fixed below the quantitative manifold; and A measuring element for measuring the pressure after the pressure balance between the sample tube and the quantitative manifold and the manifold temperature.
2. The shale reservoir space hydrophilic characteristic evaluation device under different water content conditions according to claim 1, wherein In the sample preparation area, there is a part with a fixed metal sieve plate and a telescopic vibrating grinding pestle; the telescopic vibrating grinding pestle is used to grind the sample on the top metal sieve plate, and the bottom metal sieve plate is used to collect the powdered rock sample; among them, the mesh numbers of the top metal sieve plate and the bottom metal sieve plate match the mesh number of the powdered rock sample to collect the powdered rock sample that meets the mesh number requirements.
3. The shale reservoir space hydrophilic characteristic evaluation device under different water content conditions according to claim 1, characterized in that The saturated solution area includes a solute tank and a solvent tank; in the saturated solution area, a quantitative amount of solute and solvent are added to the solution tank to prepare a solution; a stirrer is provided in the saturated solution area for stirring the solution to accelerate the relative humidity balance process in the saturated solution area.
4. The shale reservoir space hydrophilic characteristic evaluation device under different water content conditions according to claim 1, wherein The experimental area includes a sieve plate storage area; the sieve plate storage area is set as the enclosed space, and a temperature control unit for controlling the temperature in the enclosed space is provided in the enclosed space; the sieve plate storage area is adjacent to the sample preparation area, and the opening and closing door is opened on the sieve plate storage area.
5. The hydrophilic characteristic evaluation device for shale reservoir space under different water-containing conditions according to claim 4, wherein The experimental area includes a sample drying area; the sample drying area is set as the enclosed space, and a temperature control unit for controlling the temperature in the enclosed space and a telescopic robotic arm a for transferring the sample clamp from the sample drying area are provided in the enclosed space; the opening and closing door is opened on the sample drying area; the sample drying area is connected to an external vacuum pump a.
6. The hydrophilic characteristic evaluation device for shale reservoir space under different water content conditions according to claim 1, wherein The evaluation device for the hydrophilic characteristics of shale reservoir spaces under different water content conditions includes a transition area; the transition area is adjacent to at least one enclosed space in the experimental area; a control door is opened on the transition area, and the transition area is used for the transition when the sample is transferred between different enclosed spaces; a temperature control unit for controlling the temperature in the enclosed space is provided in the transition area.
7. The shale reservoir space hydrophilic characteristic evaluation device under different water content conditions according to claim 1, wherein, The evaluation device for the hydrophilic characteristics of shale reservoir spaces under different water content conditions includes a cleaning area with a control door; the cleaning area is used to receive and clean the experimental instruments that come into direct contact with the samples; the cleaning area includes a cleaning tank and a fixedly arranged ultrasonic transducer; the bottom of the cleaning tank is connected to a liquid drainer, and the liquid drainer is connected to a waste liquid collection area; the bottom of the cleaning tank is connected to a feeder, and the feeder is connected to a cleaning agent supply area.
8. The hydrophilic characteristic evaluation device for shale reservoir space under different water content conditions according to any one of claims 1-7, characterized in that The temperature control unit includes a constant temperature controller, a temperature sensor, and a heater.
9. The hydrophilic characteristic evaluation device for shale reservoir spaces under different water-containing conditions according to any one of claims 1-7, characterized in that, The gas adsorption area is connected to an external vacuum pump b; and / or, The quantitative manifold is connected to an adsorbate gas container and a free space measurement gas container.
10. The shale reservoir space hydrophilic characteristic evaluation device under different water-containing conditions according to any one of claims 1-7, characterized in that, The sample tube includes an outer sample tube; the outer sample tube has a spherical container, and the spherical container is fixedly connected with a neck; a filling column is inserted into the outer sample tube, the neck has an opening, and a sample tube opening and closing door is arranged at the opening.
11. A method for evaluating the hydrophilic characteristics of shale reservoir spaces under different water-containing conditions, characterized in that, It includes the following steps: S1. In the sample preparation area, grind the sample placed on the metal sieve template a; among them, the required mesh number of the rock powder sample is Ms1 - Ms2. There are two fixed metal sieve templates in the sample preparation area. The upper limit of the mesh number conforms to the range value Ms1 of the metal sieve template a, and the lower limit of the mesh number conforms to the range value Ms2 of the metal sieve template b. S2. The powdered rock sample that meets the mesh number requirement passes through the metal sieve template a and is concentrated on the metal sieve template b; record the mass of the rock powder sample as m1, among which, there is a micro gravity sensor attached to the metal sieve template b. S3. In the saturated solution area, add a quantitative amount of solute and solvent to the solution tank to prepare a solution, and set a preset humidity RH1; the metal sieve template b enters the saturated solution area and seals the saturated solution area until the humidity reaches RH1 again. S4. The sample transfer tank enters the saturated solution area and buckles to fix the metal sieve template b, and the sample transfer tank returns to the gas adsorption area with the metal sieve template b. S5. The sample transfer tank is flipped, and the sample drops and is collected into the sample tube; the retractable robotic arm b transfers the sample tube containing the sample to below the quantitative manifold and fixes it; coolant is added to the Dewar tank. S6. Charge the metering manifold with a quantified free space measurement gas, and record this pressure as P after equilibrium m and the manifold temperature T m ; Open the metering manifold again so that the free space measurement gas inside the metering manifold is charged into the sample tube, and record this pressure as P after the pressure reaches equilibrium m ’ and the manifold temperature T m ’ ; S7. Fill the metering manifold with the adsorbate gas. After equilibrium, record this pressure as P1 and the manifold temperature as T1. Open the metering manifold again so that the adsorbate gas inside the metering manifold fills the sample tube. After the pressure reaches equilibrium, record this pressure as P1 ’ and the manifold temperature T1 ’ ; S8. According to the free space measurement gas pressure data, the free space is determined by the linear relationship between the volume of the free space measurement gas supplied to the sample tube and the final equilibrium pressure, and there is: Where: V di is the gas supply volume of a certain data point, V di-1 is the gas supply volume of the previous data point, T std is the standard state temperature of the gas, P std is the standard state pressure of the gas, V m is the free space volume; S9. Apply V di Perform linear regression on P mi ', and the obtained slope and intercept are used to correct the free space volume and nitrogen adsorption data; where the volume of the adsorbate gas is: Where: V di is the gas supply volume at a certain data point, A F is the slope of the regression line of the free space measurement gas, B F is the intercept of the regression line of the free space measurement gas, m1 is the mass of the rock powder sample, P i ′ is the pressure when the adsorbate gas fills the sample tube and reaches equilibrium; S10. Repeat the gas adsorption experiment, and calculate the adsorption amount at each pressure point corresponding to the humidity RH1.
12. The method for evaluating the hydrophilic characteristics of shale reservoir spaces under different water-bearing conditions according to claim 11, wherein The evaluation method for the hydrophilic characteristics of shale reservoir spaces under different water content conditions includes the following steps: S11. After a certain experiment is completed, the retractable robotic arm b retrieves the sample tube and places it on the sample transfer tank. The sample transfer tank is flipped, and the sample is placed back on the metal sieve template b; set a preset temperature 1, and continuously dry the sample. S12. Drain the solution in the solution tank; according to the preset humidity RH2, by jointly controlling the solute addition port and the solvent addition port, add the solute and solvent that meet RH2 to the solution tank. S13. The metal sieve template b is transported to the saturated solution area until the humidity reaches RH2; repeat the adsorption experiment to obtain the adsorption volume V corresponding to each pressure point at RH2 2i '; S14. The adsorption experiment is repeated multiple times to obtain RH n The adsorption volume V at each corresponding pressure point ni ’; S15. Calculate the hydrophilic space parameter RW for different relative humidity stages n , Where: V' nimax is the maximum adsorption volume measured, LN(RH n ) is the natural logarithm of the relative humidity.